近红外光谱法快速测定逍遥丸(浓缩丸)中水分含量

目的: 应用近红外光谱法建立一种逍遥丸(浓缩丸)中水分含量的快速测定方法。方法: 利用烘干法测定样品中水分含量,并以其作为参考值,运用偏最小二乘法(PLS)建立水分含量与近红外光谱之间的多元校正模型,对未知样品进行含量预测。结果: 所建水分定量分析模型的相关系数(R²),校正均方差(RMSEC),预测均方差(RMSEP)分别为0.953 52,0.132,0.177。结论: 方法操作简便,无污染,结果准确可靠,可用于逍遥丸(浓缩丸)中水分含量的快速测定。     

数学模型参数在中成药固体制剂防潮中的应用

吸湿是导致中成药固体制剂质量和疗效不稳定主要原因之一,而中药成分的性质、提取纯化工艺、处方组成、包装和贮藏条件是造成中成药固体制剂吸潮的主要因素。本文应用数学模型参数总结现有的防潮技术,为中成药固体制剂防潮提供依据。     

Evaluation of Tableting and Tablet Properties of Kollidon SR: The Influence of Moisture and Mixtures with Theophylline Monohydrate

The aim of the study was firstly to investigate the influence of moisture on the tableting and tablet properties of Kollidon SR and secondly to investigate the influence of theophylline monohydrate on the tableting behavior and tablet properties produced from binary mixtures with Kollidon SR. In comparison to Kollidon SR, microcrystalline cellulose (MCC) was used. The glass transition temperature (T_g) of the powder over the whole range of RH (0–90%), and in addition, the T_g of tablets of Kollidon SR were measured. Densities and flowability of the powders were analyzed. The tablets were produced at five different maximum relative densities (ρ_{rel, max}) on an instrumented eccentric tableting machine. They were produced at three different relative humidities (RH), 30%, 45%, and 60% RH for the pure substances and binary mixtures with different ratios of drug and excipient were tableted at 45% RH. The tableting properties were analyzed by 3D modeling, force-displacement profiles, and compactibility plots. First, the T_g of the powder decreased with increasing RH and the T_g of the tablet was 4–8 K lower than the powder. The predominant deformation of Kollidon SR is plastic deformation and Kollidon SR showed a higher compactibility than MCC. The parameters of the 3D model showed an extreme change between 45 and 60% RH, and at higher RH more and more particles deformed elastically. This was confirmed by analysis of force-displacement profiles. At 60% RH, the radial tensile strength of the Kollidon SR tablets was half of the radial tensile strength at 45% RH. The reason is a higher relative energy of plastic deformation than for MCC. This results in a better utilization of the energy to deform the powder into a tablet and the exceeding of the glass transition temperature at higher RH. In conclusion, at 60% RH at the same ρ_{rel, max}, tableting and tablet properties of Kollidon SR are extremely changed since plasticity is significantly higher. In the second part of the study, the insufficient flowability of theophylline monohydrate can be compensated by using Kollidon SR in a mixture with up to 20% theophylline. Further, pressure plasticity ε of MCC and Kollidon SR was lowered in the mixture with theophylline monohydrate. The same is valid for the compactibility. The influence of theophylline monohydrate on the pressure plasticity e of the mixtures was better compensated in the mixture with MCC than in a mixture with Kollidon SR. This compensation was also visible by analyzing the force-displacement-profiles. However, hardly any influence on the radial tensile strength could be detected. Kollidon SR and Kollidon SR mixtures exhibited a higher compactibility than MCC and MCC mixtures. The differences became smaller with increasing theophylline content.     

The Nonsteady State Modeling of Freeze Drying: In-Process Product Temperature and Moisture Content Mapping and Pharmaceutical Product Quality Applications

Introduction. Theoretical models of the freeze-drying process are potentially useful to guide the design of a freeze-drying process as well as to obtain information not readily accessible by direct experimentation, such as moisture distribution and glass transition temperature, T_g, within a vial during processing. Previous models were either restricted to the steady state and/or to one-dimensional problems. While such models are useful, the restrictions seriously limit applications of the theory. An earlier work from these laboratories presented a nonsteady state, two-dimensional model (which becomes a three-dimensional model with an axis of symmetry) of sublimation and desorption that is quite versatile and allows the user to investigate a wide variety of heat and mass transfer problems in both primary and secondary drying. The earlier treatment focused on the mathematical details of the finite element formulation of the problem and on validation of the calculations. The objective of the current study is to provide the physical rational for the choice of boundary conditions, to validate the model by comparison of calculated results with experimental data, and to discuss several representative pharmaceutical applications. To validate the model and evaluate its utility in studying distribution of moisture and glass transition temperature in a representative product, calculations for a sucrose-based formulation were performed, and selected results were compared with experimental data. Theoretical Model. The model is based on a set of coupled differential equations resulting from constraints imposed by conservation of energy and mass, where numerical results are obtained using finite element analysis. Use of the model proceeds via a “modular software package” supported by Technalysis Inc. (Passage?/Freeze Drying). This package allows the user to define the problem by inputing shelf temperature, chamber pressure, container properties, product properties, and numerical analysis parameters required for the finite element analysis. Most input data are either available in the literature or may be easily estimated. Product resistance to water vapor flow, mass transfer coefficients describing secondary drying, and container heat transfer coefficients must normally be measured. Each element (i.e., each small subsystem of the product) may be assigned different values of product resistance to accurately describe the nonlinear resistance behavior often shown by real products. During primary drying, the chamber pressure and shelf temperature may be varied in steps. During secondary drying, the change in gas composition from pure water to mostly inert gas is calculated by the model from the instantaneous water vapor flux and the input pumping capacity of the freeze dryer. Results. Comparison of the theoretical results with the experiment data for a 3% sucrose formulation is generally satisfactory. Primary drying times agree within two hours, and the product temperature vs. time curves in primary drying agree within about ± 1°C. The residual moisture vs. time curve is predicted by the theory within the likely experimental error, and the lack of large variation in moisture within the vial (i.e., top vs. side vs. bottom) is also correctly predicted by theory. The theoretical calculations also provide the time variation of “T_g–T” during both primary and secondary drying, where T is product temperature and T_g is the glass transition temperature of the product phase. The calculations demonstrate that with a secondary drying protocol using a rapid ramp of shelf temperature, the product temperature does rise above Tg during early secondary drying, perhaps being a factor in the phenomenon known as “cake shrinkage”. Conclusion. The theoretical results of in-process product temperature, primary drying time, and moisture content mapping and history are consistent with the experimental results, suggesting the theoretical model should be useful in process development and “trouble-shooting” applications.     

近红外光谱用于甘草中甘草苷、甘草酸及水分测定

目的:运用近红外光谱(NIR)技术检测甘草药材中的甘草苷、甘草酸及水分。方法:采用积分球漫反射扫描近红外光谱,以TQ Analyst软件进行数据分析,建立甘草中甘草苷、甘草酸及水分测定的NIR。结果:甘草苷的预测均方根误差(RMSEP)为0.165,预测集相关系数(Rp)0.986 8;交叉验证均方根误差(RMSECV)为0.393,校正集相关系数(Rv)0.904 6。甘草酸的RMSEP=0.166,Rp=0.995 5;RMSECV=0.575,Rv=0.954 0。水分的RMSEP=0.137,Rp=0.995 2;RMSECV=0.498,Rv=0.931 9。结论:该方法快速、简便。可以用于甘草中甘草苷、甘草酸及水分的含量测定。     

近红外光谱分析技术在散结镇痛胶囊干燥过程水分检测中的应用

目的：本实验对近红外光谱（Near Infrared,NIR）分析技术在散结镇痛胶囊干燥过程中水分含量检测的可行性进行分析研究。方法：收集67批散结镇痛胶囊干燥过程不同水分含量的样品,扫描NIR光谱,分别考察比较不同波段和不同预处理方式所建立的模型的性能,最终选择1350-2030nm波段,Mean Center预处理方式,运用偏最小二乘法（PLS）建立NIRS与水分含量值之间的多元校正模型,并用此模型进行预测。结果：结果发现,选取1350-2030nm波段,Mean Center处理方式校正后建立的水分含量模型R_C=0.9950,R_V=0.9941,RMSEC=0.0096,RMSEV=0.0167,PC=4（软件根据PRESS值最小提供的主因子数）,所建立的模型较其他条件建立的模型性能更稳定,模型预测性能较优,表明样品光谱与其中水分质量分数之间存在良好的相关性。该模型对9批散结镇痛胶囊样本水分含量进行预测,R_P=0.9916,表明预测效果良好,能够满足中药生产过程中质量控制要求。结论：建立的近红外水分定量模型可以准确预测散结镇痛胶囊干燥过程水分含量,证实了NIR技术在散结镇痛胶囊干燥过程水分含量检测的可行性。     

含水量对膏滋成品保存期限的影响

目的:考察含水量对膏滋成品质量的影响.方法:按传统浓缩、收膏工艺加工生产膏滋成品,测定含水量,根据2010年版《中国药典》附录XⅢC微生物限度检查方法考察不同含水量对膏方微生物学的影响.结果:含水量对膏滋成品的微生物学影响显著,随含水量的增加,产生菌落,膏滋的稳定性降低.结论:通过严格控制膏滋的含水量,可有效地避免膏滋变硬、霉变等现象,保证膏滋成品质量同时延长保存期限.     

清瘟败毒胶囊的吸湿性研究及数据分析

目的：本实验研究清瘟败毒胶囊及其相应空胶囊的吸湿性，回归分析得到吸湿曲线方程，推测出清瘟败毒胶囊和空胶囊的临界相对湿度（CRH）。方法：测定清瘟败毒胶囊和空胶囊在四种不同相对湿度（RH）下的吸湿量，整理出清瘟败毒胶囊和空胶囊在不同RH下的吸湿曲线以及它们的CRH。结果与结论：清瘟败毒胶囊和空胶囊的CRH分别为66％和65％。     

Effect of denture adhesives on oral moisture: A multicenter randomized controlled trial

PurposeThe purpose of this study was to investigate the effect of denture adhesives on oral moisture in a 10-center parallel randomized clinical trial.MethodsTwo hundred edentulous subjects wearing complete dentures were allocated into three groups: cream-type adhesive, powder-type adhesive and control groups. The adhesives (and saline solution in the control group) were applied to the mucosal surface of the dentures for 4 days, and baseline data and data after the intervention for eight meals over 4 days were obtained. For the main outcome, oral moisture was measured with a moisture checking device. Secondary outcomes were denture satisfaction, masticatory performance, denture retention, and occlusal force. In addition to between-group and within-group comparisons of oral moisture, investigations for secondary outcomes were undertaken in subgroups classified according to the degree of oral moisture at baseline (normal subgroup and dry mouth subgroup). Intention-to-treat analysis was also performed.ResultsBetween-group and within-group comparisons of oral moisture showed no significant differences. The cream-type and powder-type denture adhesives were significantly effective in the dry mouth group for denture satisfaction ratings of ability to masticate, stability, retention, and comfort of mandibular dentures (p < 0.05). The masticatory performance and retentive force of the dry mouth denture adhesive using groups were significantly improved after intervention (p < 0.05).ConclusionsThe oral moisture of complete denture wearers was not influenced by the use of denture adhesives. Our findings showed that denture adhesives improved subjective denture satisfaction, masticatory performance, and retention for complete denture patients with oral dryness.     

润口液药理作用及刺激性的研究

润口液是一种用于解除生理性、病理性口干的制剂。实验研究结果表明，润口液具有促进唾液分泌，保持口腔湿润的功能，并且无毒、无刺激性。